CN104439259B - The preparation method of the spherical passivation alloy welding powder of a kind of short flow process - Google Patents
The preparation method of the spherical passivation alloy welding powder of a kind of short flow process Download PDFInfo
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Abstract
The present invention relates to the preparation method of the spherical passivation alloy welding powder of a kind of short flow process, belong to soft solder and manufacture field. Each raw material required solder alloy are prepared burden according to percentage by weight, and drop into smelting furnace, smelting furnace carries out forvacuum processing, is filled with inert protective gas; Be heated to the temperature of the above 30-150 of solder liquidus curve DEG C, fusing obtains alloy molten solution, and stirs; Spray chamber is carried out, after forvacuum processing, being filled with inert gas to normal pressure, then pass into the reacting gas of atomization process; Utilize woven hose that alloy molten solution is evenly delivered to atomizer, make alloy molten solution be atomized into fine droplet at spray chamber, this droplet in flight, nodularization and cooling, process of setting with spray chamber in reacting gas directly there is chemical action, obtain passivation layer; Classification; Packaging, warehouse-in. The method is applicable to the passivation of various atomization methods and each alloy welding powder that becomes to be grouped into, particularly better for the effect of oxidizable alloy welding powder or fine welding powder.
Description
Technical field
The present invention relates to the preparation method of the spherical passivation alloy welding powder of a kind of short flow process, particularly a kind of spherical alloyThe short flow process passivating method of dry method of welding powder, belongs to soft solder manufacturing technology field.
Background technology
Alloy welding powder is owing to having less particle diameter, and higher specific area and higher surface energy, be easy to by skyIn dioxygen oxidation in gas and welding use procedure, occur tin sweat(ing), this has brought very large to storage and the use of welding powderUnfavorable. Particularly, along with the appearance of VHD integrated circuit, the particle size of required alloy welding powder becomes more and moreLittle, and scolder unleaded since, the worse lead-free alloy welding powder of a large amount of oxidative resistances occurs, its surface stableProperty keeps just seeming even more important. On close spacing device, carry out that paste solder printing is must used thickness thinner, perforate moreLittle web plate, this alloy welding powder granularity that has just determined tin cream used is thinner. If do not use fine powder tin cream, canThe direct result that can cause is exactly that minimizing and the tin amount of tin amount under paste solder printing is inconsistent, and tin cream is difficult for from web plate simultaneouslyThe demoulding. Alloy welding powder is being made after soldering paste, and active component in solder flux easily and the alloy of top layer unpassivated processingWelding powder reacts, and causes soldering paste to use the unstable of viscosity and storage viscosity, even occur dry, send out phenomenon husky,Affect printing/application use and the postwelding quality of welding spot of soldering paste.
Passivation welding powder can play and improve welding powder mobility, suppresses micro mist and reunites, and improves non-oxidizability, extends welding powderShelf-life, stop the effect reacting with scaling powder. The passivating method of having reported is mainly organic coating, workSkill comprises infusion process, spraying process, vapor deposition process and ball-milling method, and these methods are mainly with after preparing at welding powder,Be coated by welding powder being carried out to secondary in subsequent technique, inevitable like this having increased introduced new impurity and process increasingThe chance of oxygen, and increased equipment and human input; In addition, increase operational sequence, extended production technology streamJourney, reduces production efficiency, and the stability control difficulty of product quality increases. Wherein again taking infusion process as main, as,In Chinese patent 95117301.4, disclose covering has been dissolved in to a kind of solvent, then, by metal alloy powder dipping bath, putAfter falling liquation, powder is placed and spent the night in 60 DEG C of baking ovens, obtain the coated thickness of 100 molecular layers; Chinese patent99810452.3 disclose after solder powder is stirred to certain hour in stearic acid saturated solution and separate and be dried, orReduce the saturation degree of acylate by splashing into alcohols, be coated on welding powder surface after it is separated out; Chinese patent101767198 utilize Ultrasound Instrument ultrasonic vibration series leadless solder alloy powder, are scattered in deployed stearic acid wineIn essence solution, and must be coated fine and close modification solder alloy powder after suction filtration is dry; Chinese patent 101745636Adopt and immerse prewired active organic solvent, then through the dry mode of drip washing. And Chinese patent 95117301.4 is by goldBelong to alloy powder on a large surface, spread out, then by covering solution spraying on powder, final powder warpThe dry coated composite powder that obtains; In Chinese patent 93103095.1 by the steam (400-750 DEG C to xylylene dimerLower formation activated monomer) be sent to the settling chamber of the rotating cylinder that is loaded with welding powder, make xylylene monomer vapours existWelding powder surface condensation, forms polymer or copolymer film; Chinese patent 99801693.4 has been gasificated into organic acidAfter machine steam, utilize the welding powder surface chemical reaction that itself and classification are good to form passivation layer. Iwasaki etc. adopt alloyThe method of raw material and the common ball milling of organic coating agent has obtained the Sn-Zn that top layer is coated with 12-hydroxy stearic acid and has been associated goldWelding powder, but this method is difficult to obtain desirable spherical passivation welding powder.
Desirable passivation should realize in the production process of welding powder, like this can welding powder form at first fundamentallyReach passivation object, be also convenient to follow-up separation and the packaging of welding powder; Between dielectric passivation and welding powder preferably with chemical bondForm combination, passivator consumption is few and can not dissolved by scaling powder like this, passivation welding powder can stable existence in soldering pasteIn, and can not affect the quality of soldering paste.
But regrettably about in alloy atomization process, the short flow process passivation that utilizes gas to react online with molten dropCoating technology has no relevant report in this area. There is document announcement, micro-by directly adding in alloy melting processAmount oxidation-resistant alloy element, belongs to short flow process passivating technique, can draw but add anti-oxidant element in alloy molten solutionPlay the variation of physical property after gold alloy solder, what is more important, the preparation method of general alloy welding powder all adopts and hasThe atomization method (comprising aerosolization, centrifugal atomizing, ultrasonic atomizatio) of rapid solidification features, in the time of atomization, alloy is micro-Anti-oxidant element in dripping has little time to be enriched in particle surface and forms desirable passivation layer, causes the passivation effect of welding powderPoor. Gas reacts passivating technique online, belongs to reaction and the enrichment on molten drop top layer, has avoided alloy raw material insidePollution, its most critical point is to utilize the concentration of reacting gas and the control of temperature and atomization temperature, makes alloy moltenDrop in the good reaction passivation layer of formation in the short time in nodularization process.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, a kind of spherical alloy welding powder is providedThe short flow process passivating method of dry method, belongs to the dry method passivation of alloy welding powder. Make it in the advantage that keeps welding powder passivation effectOn basis, eliminate the operations such as cleaning in the coated process of conventional welding powder wet method-coated-dry, shorten welding powder passivationFlow process, reduce passivation cost, promoted production efficiency, be convenient to suitability for industrialized production. Meanwhile, avoid process pollute,Improving The Quality of Products, the follow-up classification that effectively solves welding powder is selected/sieves and store oxidation and prepares, stores at solder(ing) pasteThe instability problem of lotion viscosity, printing in process, reduces postwelding tin sweat(ing) incidence, promotes soldering wetability.
For achieving the above object, the present invention takes following technical scheme:
A preparation method for the spherical passivation alloy welding powder of short flow process, comprises the following steps:
1) each raw material required solder alloy are prepared burden according to percentage by weight, and each raw material are dropped into meltingStove, smelting furnace carries out forvacuum processing, is then filled with inert protective gas;
2) by step 1) in each raw material be heated to the temperature of the above 30-150 of solder alloy liquidus curve DEG C, fusingObtain alloy molten solution, and stir;
3) spray chamber is carried out, after forvacuum processing, being filled with inert gas to normal pressure, then pass into atomization processReacting gas, and make it to keep uniform temperature and concentration range;
4) utilizing woven hose by step 2) alloy molten solution of gained is evenly delivered to atomizer, adjusts atomizer parameter,Making solder alloy liquation in step 3) described spray chamber is atomized into the fine droplet of clean appearance, and this droplet is flyingIn row, nodularization and cooling, process of setting with spray chamber in reacting gas directly issue biochemical in higher temperatureEffect, obtains desirable passivation layer, thereby prepares the former powder of passivation alloy welding powder;
5) by step 4) the classified system level of passivation alloy welding powder of gained, obtain have certain particle size range andThe spherical welding powder distributing;
6) after end product quality detects, by step 5) the classified qualified spherical passivation alloy welding powder that obtains,After vacuumizing or vacuumizing, be filled with inert gas to micro-negative pressure packaging, warehouse-in.
Step 1) in, smelting furnace is evacuated to 1 × 10-2-1×10-1Pa, be filled with inert protective gas after pressure be0.2-0.5MPa, described inert protective gas is nitrogen or argon gas.
Step 2) in, described alloy molten solution be Sn-Pb, Sn-Pb-Ag, Sn-Pb-Bi, Sn-Cu, Sn-Ag,Sn-Ag-Cu, Sn-Zn, Sn-Bi, Sn-Bi-Ag, Sn-Bi-Cu alloy system, the stirring means of alloy molten solution is lazyProperty protective gas stir or mechanical agitation, 20min-4h.
Step 3) in, spray chamber forvacuum to 1 × 10-2-1×10-1Pa, is then filled with nitrogen or argon gas to normal pressure,And make spray chamber temperature range at 40-150 DEG C by temperature controlling instruments.
The reacting gas of described atomization process is oxidizing gas or organic steam, and its concentration is controlled at10-50000ppm scope.
Oxidative reaction gas is F preferably2、Cl2、Br2、O2, its concentration is controlled at 10-3000ppm.
Organic reaction gas is 12-hydroxy stearic acid, benzoic acid, acetylacetone,2,4-pentanedione, acetic acid (acetic acid), second two preferablyAcid steam, its concentration range is 1000-50000ppm, that is: 0.1%-5vol%, organic steam by heating orThe method that high-frequency ultrasonic atomization or high-temperature gas carry obtains.
Step 4) in, in woven hose, the feed flow of alloy molten solution is 20-150kg/h, described atomizer is aerosolChange the ultrasonic head of nozzle, centrifugal atomizing dish or power ultrasonic atomization.
Step 5) in, described hierarchy system is online selection by winnowing, off-line vibrosieve, or selection by winnowing and vibrosieveCombined classification system, trimmed size welding powder be T3 (25-45 μ m), T4 (20-38 μ m), T5 (15-25 μ m),T6 (5-15 μ m), T7 (2-11 μ m) or T8 (2-8 μ m).
In this method, described inert protective gas or inert gas are nitrogen or argon gas.
The present invention in the atomization process of alloy welding powder, by passing into online quantitative oxidizing gas or organic steam,Utilize the clean pyrosol in surface to drop in on-line oxidation reaction in solidification process or the method for organic compound, makeAlloy welding powder surface forms thin and fine and close oxide-film or the organic protective film of one deck. Be applicable to various atomization methods and eachBecome the passivation of the alloy welding powder that is grouped into, particularly for the effect of oxidizable alloy welding powder or fine welding powder moreGood.
Advantage of the present invention is by controlling concentration and the temperature of atomization reaction atmosphere in alloy welding powder atomization preparation processDegree, makes clean alloy droplet its surface in the time of liquid high temperature, with atomization indoor gas, chemical action directly occur,And utilize the interfacial tension effect of alloy droplet in the time of different atmosphere, make alloy micro-by the adjustment control of atomization temperatureDrip nodularization, solidify, the online short flow process passivation that has realized spherical welding powder is coated, has eliminated the coated needs of welding powder wet methodAfter being prepared into welding powder, cleaning-be coated-dry techniqueflow, reduced passivation cost, promoted production efficiency, withTime avoided process pollution, promoted product quality, be convenient to suitability for industrialized production.
The present invention efficiently solves follow-up classification choosing/screening and storage oxidation and easy the showing of reuniting of fine welding powder of welding powderResemble, avoided the instability problem of lotion viscosity, printing in solder(ing) paste preparation, storing process, use this welderingSolder(ing) paste prepared by powder without refrigeration, viscosity stabilization, can not produce and dryly send out phenomenon husky, postwelding tin sweat(ing) is few, wettingProperty is good. Be specially adapted to oxidizable alloy welding powder and high speed printing field high stability solder(ing) paste and VHDThe preparation of welding powder for the ultra-fine tin cream in assembling field.
Below by the drawings and specific embodiments, the present invention will be further described, but and do not mean that the present inventionThe restriction of protection domain.
Brief description of the drawings
Fig. 1 is the embodiment of the present invention T4 type (Cl of 20-38 μ Sn-3.0Ag-0.5Cu alloy m)2After passivation, weldPowder SEM pattern photo.
Fig. 2 is the Sn-37Pb welding powder IR (infared spectrum) of embodiment of the present invention 12-hydroxy stearic acid steam passivation.
Detailed description of the invention
Embodiment 1
(25-45 μ is type F m) for the T3 of Sn-58Bi alloy2The ultrasonic atomizatio preparation method of passivation welding powder, comprises following stepRapid:
1) pure Sn required Sn-58Bi solder alloy and pure Bi raw material are joined according to percentage by weight 42:58 ratioMaterial, and two kinds of raw material are dropped into smelting furnace simultaneously, then smelting furnace is evacuated to 1 × 10-2After Pa, be filled with nitrogenGas (N2) to pressure be 0.2MPa;
2) smelting furnace is heated to the solder liquidus curve temperature of 100 DEG C above, 238 DEG C, makes raw material fusingBecome alloy molten solution, and pass into nitrogen (N2) stir 20min;
3) to ultrasonic atomizatio chamber carry out forvacuum to 1 × 10-2After Pa, be filled with nitrogen (N2) to normal pressure, then logicalEnter F2Gas, and make F2Concentration remains on 10ppm left and right, and controls spray chamber temperature 40 DEG C of left and right;
4) utilize woven hose that above-mentioned Sn-58Bi alloy molten solution is evenly delivered to the super of spray chamber with the flow of 20kg/hSound head, adjusts atomizer parameter and makes solder alloy liquid stream on atomizer, stablize atomization, preparation F2The gold alloy solder of passivationExpect former powder;
5) the former powder of above-mentioned collection is put on ultrasonic vibration screening machine and carries out vibrosieve, vibrating screen classifier isThe vibrating screen classifier of upper 325 orders, lower 500 order Double-layer screens, obtains T3 (m) welding powder of 25-45 μ.
6) above-mentioned T3 welding powder is carried out to the tests such as composition, granularity, pattern, tin sweat(ing), vacuumize also after qualifiedBe filled with nitrogen to micro-negative pressure packaging, and record warehouse-in.
Embodiment 2
(15-25 μ is type Br m) for the T5 of Sn-57Bi-1Ag alloy2The centrifugal atomizing preparation method of passivation welding powder, comprisesFollowing steps:
1) pure Sn required Sn-57Bi-1Ag solder alloy, pure Bi and SnAg10 intermediate alloy raw material are pressedAccording to percentage by weight batching, and each raw material are dropped into smelting furnace, then smelting furnace is evacuated to 1 × 10-2After Pa,Being filled with argon gas (Ar) to pressure is 0.5MPa;
2) above-mentioned each raw material are heated to the solder liquidus curve temperature of 30 DEG C above, 168 DEG C, make itBe fused into alloy molten solution, and argon gas (Ar) stirs 4 hours;
3) to centrifugal atomizing chamber carry out forvacuum to 1 × 10-2After Pa, be filled with argon gas (Ar) to normal pressure, thenPass into the Br of 100 DEG C2Gas, and make it to remain on 3000ppm left and right, control spray chamber temperature and maintain 100 DEG CLeft and right;
4) utilize woven hose that above-mentioned Sn-57Bi-1Ag alloy molten solution is evenly delivered to atomization with the flow of 150kg/hThe centrifugal atomizing dish of chamber, adjusts atomizing disk rotating speed and makes solder alloy liquid stream on atomizer, stablize atomization, preparation Br2The alloy welding powder of passivation;
5) utilize online selection by winnowing hierarchy system to carry out real-time selection by winnowing, after Ultramicro-powder is separated with super meal, place separately,Then the qualified welding powder at nearly end of having rejected Ultramicro-powder and super meal is put in to 500 order/800 of ultrasonic vibration screening machineOn order Double-layer screen, carry out vibrosieve, obtain T5 (m) welding powder of 15-25 μ.
6) above-mentioned T5 welding powder carry out composition, granularity, pattern, tin sweat(ing) test all qualified after, after vacuumizing, fillEnter argon gas and pack and record warehouse-in.
Embodiment 3
T4 type (m) the Cl of 20-38 μ of Sn-3.0Ag-0.5Cu alloy2The centrifugal atomizing preparation method of welding powder after passivation,Comprise the following steps:
1) by the middle of pure Sn required Sn-3.0Ag-0.5Cu solder alloy, SnCu20 intermediate alloy and SnAg10Alloy raw material amounts to 100kg prepares burden according to percentage by weight, and each raw material are dropped into smelting furnace, then will meltFurnace is evacuated to 1 × 10-1After Pa, be filled with nitrogen (N2) to pressure be 0.5MPa;
2) above-mentioned each raw material are heated to the solder liquidus curve temperature of 80 DEG C above, 297 DEG C, make itBe fused into alloy molten solution, and nitrogen (N2) stir 2 hours;
3) to centrifugal atomizing chamber carry out forvacuum to 1 × 10-1After Pa, be filled with nitrogen (N2) to normal pressure, thenPass into Cl2Gas, and make it to remain on 1000ppm left and right, control spray chamber temperature and maintain 50 DEG C of left and right;
4) utilize woven hose that above-mentioned Sn-3.0Ag-0.5Cu alloy molten solution is evenly delivered to mist with the flow of 100kg/hChange the centrifugal atomizing dish of chamber, adjust atomizing disk rotating speed and make solder alloy liquid stream on atomizer, stablize atomization, preparation Cl2The alloy welding powder of passivation;
5) utilize online selection by winnowing hierarchy system to carry out real-time selection by winnowing, after Ultramicro-powder is separated with super meal, place separately,Then the qualified welding powder at nearly end of having rejected Ultramicro-powder and super meal is put in to 400 order/700 of ultrasonic vibration screening machineOn order Double-layer screen, carry out vibrosieve, obtain T4 (m) welding powder of 20-38 μ.
6) above-mentioned T4 welding powder carry out composition, granularity, pattern, tin sweat(ing) test all qualified after, after vacuumizing, fillEnter nitrogen packed and record warehouse-in.
As shown in Figure 1, the T4 type (Cl of 20-38 μ Sn-3.0Ag-0.5Cu alloy m) for preparing2After passivationWelding powder SEM pattern photo, can find out: it is impaired that selection by winnowing classification and sieve classification all do not cause that passivation layer destroys,Passivation layer is firm; Welding powder after passivation is spherical in shape, and passivation atmosphere does not impact powder sphericity index.
Embodiment 4
T4 type (m) the O of 20-38 μ of Sn-0.7Cu alloy2After passivation, the centrifugal atomizing preparation method of welding powder, comprisesFollowing steps:
1) pure Sn required Sn-0.7Cu solder alloy and SnCu20 intermediate alloy raw material being amounted to 100kg pressesAccording to percentage by weight batching, and each raw material are dropped into smelting furnace, then smelting furnace is evacuated to 1 × 10-1After Pa,Be filled with nitrogen (N2) to pressure be 0.5MPa;
2) above-mentioned each raw material are heated to the solder liquidus curve temperature of 80 DEG C above, 307 DEG C, make itBe fused into alloy molten solution, and nitrogen (N2) stir 4 hours;
3) to centrifugal atomizing chamber carry out forvacuum to 1 × 10-1After Pa, be filled with nitrogen (N2) to normal pressure, thenPass into O2Gas, and make it to remain on 100ppm left and right, control spray chamber temperature and maintain 60 DEG C of left and right;
4) utilize woven hose that above-mentioned Sn-0.7Cu alloy molten solution is evenly delivered to spray chamber with the flow of 80kg/hCentrifugal atomizing dish, adjusts atomizing disk rotating speed and makes solder alloy liquid stream on atomizer, stablize atomization, preparation O2PassivationAlloy welding powder;
5) utilize the hierarchy system of online selection by winnowing+screen(ing) machine to carry out choosing point in real time, wherein the screen cloth of screen(ing) machine is upper 400 ordersWith lower 700 order Double-layer screens, obtain T4 (m) welding powder of 20-38 μ.
6) above-mentioned T4 welding powder carry out composition, granularity, pattern, tin sweat(ing) test all qualified after, after vacuumizing, fillEnter nitrogen packed and record warehouse-in.
Embodiment 5
(5-15 μ is the centrifugal atomizing preparation side of welding powder after the 12-hydroxy stearic acid passivation of Sn-37Pb alloy m) for T6 typeMethod, comprises the following steps:
1) pure Sn required Sn-37Pb solder alloy and pure Pb alloy raw material are amounted to 100kg according to weightPercentage batching, and each raw material are dropped into smelting furnace, then smelting furnace is evacuated to 1 × 10-1After Pa, be filled withNitrogen (N2) to pressure be 0.2MPa;
2) above-mentioned each raw material are heated to the solder liquidus curve temperature of 120 DEG C above, 303 DEG C, make itBe fused into alloy molten solution, and nitrogen (N2) stir 2 hours;
3) to centrifugal atomizing chamber carry out forvacuum to 1 × 10-2After Pa, be filled with nitrogen (N2) to normal pressure, thenUtilize technical grade high frequency humidifier by the liquid 12-hydroxy stearic acid atomization of 120 DEG C, and make 12-hydroxyl in spray chamberStearic acid vapour concentration remains on 1000ppm (being 0.1vol%) left and right, and temperature maintains 120 DEG C of left and right;
4) utilize woven hose that above-mentioned Sn-37Pb alloy molten solution is evenly delivered to spray chamber with the flow of 100kg/hCentrifugal atomizing dish, adjusts atomizing disk rotating speed and makes solder alloy liquid stream on atomizer, stablize atomization, preparation 12-hydroxylThe alloy welding powder of stearic acid passivation;
5) air quantity and the wind speed of adjusting online selection by winnowing hierarchy system carry out real-time selection by winnowing, and (5-15 μ m) to obtain T6 typeWelding powder.
6) above-mentioned T6 welding powder carry out composition, granularity, pattern, tin sweat(ing) test all qualified after, vacuumize packagingAnd record warehouse-in.
Embodiment 6
T7 type (2-11 μ is the centrifugal atomizing preparation method of welding powder after the benzoic acid passivation of Sn-36Pb-2Ag alloy m),Comprise the following steps:
1) pure Sn required Sn-36Pb-2Ag solder alloy, pure Pb and SnAg10 intermediate alloy raw material are total toMeter 100kg prepares burden according to percentage by weight, and each raw material are dropped into smelting furnace, then smelting furnace is evacuated to1×10-1After Pa, be filled with nitrogen (N2) to pressure be 0.2MPa;
2) above-mentioned each raw material are heated to the solder liquidus curve temperature of 150 DEG C above, 333 DEG C, make itBe fused into alloy molten solution, and nitrogen (N2) stir 2 hours;
3) to centrifugal atomizing chamber carry out forvacuum to 1 × 10-2After Pa, be filled with nitrogen (N2) to normal pressure, thenUtilize high frequency humidifier by the liquid phenenyl formic acid atomization of 150 DEG C, and utilize the nitrogen of 150 DEG C by the benzoic acid of atomizationSteam is carried into spray chamber, makes the benzoic acid vapour concentration in atomization chamber remain on 10000ppm (being 1.0vol%)Left and right, maintains spray chamber temperature 150 DEG C of left and right;
4) utilize woven hose that above-mentioned Sn-37Pb alloy molten solution is evenly delivered to spray chamber with the flow of 100kg/hCentrifugal atomizing dish, adjusts atomizing disk rotating speed and makes solder alloy liquid stream on atomizer, stablize atomization, prepares benzoic acid bluntThe alloy welding powder of changing;
5) air quantity and the wind speed of adjusting online selection by winnowing hierarchy system carry out real-time selection by winnowing, and (2-11 μ m) to obtain T7 typeWelding powder.
6) above-mentioned T7 welding powder carry out composition, granularity, pattern, tin sweat(ing) test all qualified after, vacuumize packagingAnd record warehouse-in.
Embodiment 7
(25-45 μ is the argon gas atomization production of welding powder after the acetylacetone,2,4-pentanedione passivation of Sn-9Zn alloy m), bag for T3 typeDraw together following steps:
1) pure Sn required Sn-9Zn solder alloy and pure Zn raw material are amounted to 100kg according to percentage by weightBatching, and each raw material are dropped into smelting furnace, then smelting furnace is evacuated to 1 × 10-1After Pa, be filled with argon gas extremelyPressure is 0.2MPa;
2) above-mentioned each raw material are heated to the solder liquidus curve temperature of 150 DEG C above, 349 DEG C, make itBe fused into alloy molten solution, and argon gas stirs 2 hours;
3) to spray chamber carry out forvacuum to 1 × 10-2After Pa, be filled with argon gas to normal pressure, then make acetylacetone,2,4-pentanedioneEvaporation at 150 DEG C, and utilize the argon gas of 150 DEG C that steam is carried into spray chamber, make the acetyl in atomization chamberAcetone steam concentration remains on 50000ppm (being 5vol%) left and right, and spray chamber temperature is 50 DEG C of left and right;
4) utilize woven hose that above-mentioned Sn-9Zn alloy molten solution is evenly delivered to aerosolization spray with the flow of 150kg/hMouth, with high speed argon stream, liquid stream is broken and form and stablize atomization, prepare the alloy welding powder of acetylacetone,2,4-pentanedione passivationFormer powder;
5) former gained powder is evenly delivered on the ultrasonic vibration screening machine of 325 order/500 order Double-layer screens and carries outVibrosieve, (25-45 μ is Sn-9Zn passivation welding powder m) to obtain T3.
6) above-mentioned T3 welding powder carry out composition, granularity, pattern, tin sweat(ing) test all qualified after, vacuumize and fillEnter argon gas to micro-negative pressure and pack and record warehouse-in.
Embodiment 8
(2-8 μ is the centrifugal atomizing system of welding powder after the acetic acid of Sn-4.0Ag-0.5Cu alloy (acetic acid) passivation m) for T8 typePreparation Method, comprises the following steps:
1) by required Sn-4.0Ag-0.5Cu solder alloy pure Sn, SnCu10 and the former material of SnAg20 intermediate alloyMaterial amounts to 100kg prepares burden according to percentage by weight, and each raw material are dropped into smelting furnace, then smelting furnace is taken out veryEmpty to 1 × 10-2After Pa, be filled with nitrogen (N2) to pressure be 0.25MPa;
2) above-mentioned each raw material are heated to the solder liquidus curve temperature of 130 DEG C above, make it to be fused into alloyLiquation, and nitrogen (N2) stir 1 hour;
3) to spray chamber carry out forvacuum to 1 × 10-2After Pa, be filled with nitrogen to normal pressure, then make acetic acid at 120 DEG CLower gasification, and evenly pass into spray chamber, making the interior acetic acid vapour concentration of atomization chamber remain on 20000ppm (is 2vol%) left and right, spray chamber temperature maintains 80 DEG C of left and right;
4) utilize woven hose that above-mentioned Sn-4.0Ag-0.5Cu alloy molten solution is evenly delivered to mist with the flow of 50kg/hChange the centrifugal atomizing dish of chamber, adjust atomizing disk rotating speed and make solder alloy liquid stream on atomizer, stablize atomization, prepare vinegarThe alloy welding powder of acid passivation;
5) air quantity and the wind speed of adjusting online selection by winnowing hierarchy system carry out real-time selection by winnowing, and (2-8 μ m) to obtain T8 typeWelding powder.
6) above-mentioned T8 welding powder carry out composition, granularity, pattern, tin sweat(ing) test all qualified after, vacuumize packagingAnd record warehouse-in.
Embodiment 9
T4 type (20-38 μ is the centrifugal atomizing preparation method of welding powder after the ethanedioic acid passivation of Sn-30Bi-0.5Cu alloy m),Comprise the following steps:
1) by pure Sn required Sn-30Bi-0.5Cu solder alloy, pure Bi and SnCu20 intermediate alloy raw materialAmount to 100kg and prepare burden according to percentage by weight, and each raw material are dropped into smelting furnace, then smelting furnace is vacuumizedTo 1 × 10-2After Pa, be filled with nitrogen (N2) to pressure be 0.3MPa;
2) above-mentioned each raw material are heated to the solder liquidus curve temperature of 120 DEG C above, make it to be fused into alloyLiquation, and utilize and carry out mechanical agitation 1 hour with the mechanical pump of screw;
3) to spray chamber carry out forvacuum to 1 × 10-1After Pa, be filled with nitrogen to normal pressure, then utilize technical gradeHigh frequency atomizer is the liquid ethanedioic acid atomization of 120 DEG C, and 12-hydroxy stearic acid vapour concentration in spray chamber is keptIn 40000ppm (being 4vol%) left and right, temperature maintains 120 DEG C of left and right;
4) utilize woven hose that above-mentioned Sn-30Bi-0.5Cu alloy molten solution is evenly delivered to atomization with the flow of 80kg/hThe centrifugal atomizing dish of chamber, adjusts atomizing disk rotating speed and makes solder alloy liquid stream on atomizer, stablize atomization, preparation second twoThe alloy welding powder of acid passivation;
5) utilize the hierarchy system of online selection by winnowing+vibrosieve to carry out choosing point in real time, in assorting room, utilize wind-force to incite somebody to actionAfter Ultramicro-powder blows away, do return collecting, then utilize powder conveying system by gained welding powder be directed into have 325 orders andOn the ultrasonic vibration screening machine of 500 order Double-layer screens, get 325 orders and the direct welding powder of 500 orders as T3(m) welding powder of 25-45 μ.
6) above-mentioned T3 welding powder carry out composition, granularity, pattern, tin sweat(ing) test all qualified after, after vacuumizing, fillEnter nitrogen packed and record warehouse-in.
Welding powder passivation effect test experiments:
1, change color is observed:
Take gained passivation welding powder 50g, be laid on the filter paper of Φ 100mm, filter paper is placed in the flat board heating of 60 DEG COn stove, observe different welding powders change color in time, the welding powder change color of composition of the same race and granularity is significantly bluntChange weak effect.
2, tin sweat(ing) test:
Welding powder is preserved in 50 DEG C of baking ovens, got the same alloy composition of different holding times and the welding powder of granularity, useThe scaling powder preparation tin cream of the same race of identical metering, does tin sweat(ing) with identical reflux technique and tests, and observes tin sweat(ing) number, tinThe welding powder passivation effect that pearl is many is poor.
Table 1 is embodiment of the present invention solder alloy powder and contrast solder alloy powder antioxygenic property comparison and tin creamTin sweat(ing) comparison.
The non-oxidizability comparison of table 1 passivation solder alloy welding powder and non-passivation alloy welding powder
3, infrared absorption spectrum analysis
The Sn-37Pb weldering of the 12-hydroxy stearic acid steam passivation of preparing for the embodiment of the present invention 5 as shown in Figure 2,Powder IR. The characteristic absorption peak that has occurred methyl, methylene and carbonyl in the infared spectrum of passivation welding powder, illustrates welding powderSurface has absorbed 12-hydroxy stearic acid really, has formed passivation clad.
The present invention by controlling concentration and the temperature of atomization reaction atmosphere, makes to close in alloy welding powder atomization preparation processDirectly there is chemical action in gold droplet surface and spray chamber gas, has realized the online short flow process passivation bag of spherical welding powderCover, eliminated that welding powder wet method is coated need to be prepared into clean-coated-dry techniqueflow after welding powder, reduced bluntChange into this, promoted production efficiency, avoided process pollution simultaneously, promoted product quality, be convenient to industrialization rawProduce. The present invention efficiently solves follow-up classification choosing/screening and the storage oxidation of welding powder and prepares, stored at solder(ing) pasteThe instability problem of lotion viscosity, printing in journey, the solder(ing) paste that uses this welding powder to prepare is steady without refrigeration, viscosityFixed, can not produce and dryly send out phenomenon husky, postwelding tin sweat(ing) is few, wetability good. Be specially adapted to oxidizable gold alloy solderThe system of the ultra-fine tin cream welding powder in high stability solder(ing) paste and VHD assembling field for powder and high speed printing fieldStandby.
Claims (10)
1. a preparation method for the spherical passivation alloy welding powder of short flow process, comprises the following steps:
1) each raw material required solder alloy are prepared burden according to percentage by weight, and drop into smelting furnace, smelting furnaceCarry out forvacuum processing, be then filled with inert protective gas;
2) be heated to the temperature of the above 30-150 of solder alloy liquidus curve DEG C, fusing obtains alloy molten solution, and stirsEvenly;
3) spray chamber is carried out, after forvacuum processing, being filled with inert gas to normal pressure, then pass into atomization processReacting gas;
4) utilize woven hose that alloy molten solution is evenly delivered to atomizer, make solder alloy liquation in spray chamber atomizationBecome fine droplet, this small droplet in flight, nodularization and cooling, process of setting with spray chamber in reacting gasDirectly there is chemical action, obtain passivation layer, obtain the former powder of passivation alloy welding powder;
5) by the classified system level of former powder of the passivation alloy welding powder of gained;
6), after end product quality detects, after vacuumizing or vacuumizing, be filled with inert gas to micro-negative pressure packaging, warehouse-in.
2. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 1, is characterized in that:Described smelting furnace is evacuated to 1 × 10-2-1×10-1Pa, being filled with pressure after inert protective gas is 0.2-0.5MPa.
3. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 1, is characterized in that:Described alloy molten solution be Sn-Pb, Sn-Pb-Ag, Sn-Pb-Bi, Sn-Cu, Sn-Ag, Sn-Ag-Cu, Sn-Zn,Sn-Bi, Sn-Bi-Ag or Sn-Bi-Cu alloy system, the stirring means of described alloy molten solution is inert protective gasStir or mechanical agitation.
4. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 1, is characterized in that:Described spray chamber forvacuum to 1 × 10-2-1×10-1Pa, the temperature of described spray chamber is 40-150 DEG C.
5. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 1, is characterized in that:The reacting gas of described atomization process is oxidizing gas or organic steam, and its concentration is 10-50000ppm.
6. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 5, is characterized in that:Described oxidizing gas is F2、Cl2、Br2Or O2, its concentration is 10-3000ppm.
7. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 5, is characterized in that:Described organic steam is 12-hydroxy stearic acid, benzoic acid, acetylacetone,2,4-pentanedione, acetic acid (acetic acid) or ethanedioic acidSteam, its concentration range is 1000-50000ppm.
8. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 7, is characterized in that:The method that described organic steam carries by heating, high-frequency ultrasonic atomization or high-temperature gas obtains.
9. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 1, is characterized in that:In woven hose, the feed flow of alloy molten solution is 20-150kg/h, and described atomizer is aerosolization nozzle, centrifugal mistThe ultrasonic head of change dish or power ultrasonic atomization.
10. the preparation method of the spherical passivation alloy welding powder of short flow process according to claim 1, is characterized in that:Described hierarchy system is online selection by winnowing, off-line vibrosieve, or the combined classification system of selection by winnowing and vibrosieve,Finished product welding powder specification is 25-45 μ m, 20-38 μ m, 15-25 μ m, 5-15 μ m, 2-11 μ m or 2-8 μ m.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63200828A (en) * | 1987-02-17 | 1988-08-19 | Itsuo Onaka | Production of powder |
| CN1559696A (en) * | 2004-02-18 | 2005-01-05 | 王崇琳 | Preparation method of low oxygen content microballon parent metal powder and its special equipment |
| WO2009111932A1 (en) * | 2008-03-13 | 2009-09-17 | 浙江省冶金研究院有限公司 | Lead-free high-temperature electronic solder and preparing method thereof |
| CN202239638U (en) * | 2011-07-22 | 2012-05-30 | 东莞永安科技有限公司 | Improved solder powder preparation machine |
| CN102814595A (en) * | 2012-05-05 | 2012-12-12 | 大连理工大学 | Sn-Zn based near-eutectic lead-free solder alloy for aluminum-bronze soft soldering and preparation method |
| CN102909387A (en) * | 2012-11-14 | 2013-02-06 | 曹艺 | Preparation method for metal injection molding alloy powder |
-
2014
- 2014-11-25 CN CN201410691248.7A patent/CN104439259B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63200828A (en) * | 1987-02-17 | 1988-08-19 | Itsuo Onaka | Production of powder |
| CN1559696A (en) * | 2004-02-18 | 2005-01-05 | 王崇琳 | Preparation method of low oxygen content microballon parent metal powder and its special equipment |
| WO2009111932A1 (en) * | 2008-03-13 | 2009-09-17 | 浙江省冶金研究院有限公司 | Lead-free high-temperature electronic solder and preparing method thereof |
| CN202239638U (en) * | 2011-07-22 | 2012-05-30 | 东莞永安科技有限公司 | Improved solder powder preparation machine |
| CN102814595A (en) * | 2012-05-05 | 2012-12-12 | 大连理工大学 | Sn-Zn based near-eutectic lead-free solder alloy for aluminum-bronze soft soldering and preparation method |
| CN102909387A (en) * | 2012-11-14 | 2013-02-06 | 曹艺 | Preparation method for metal injection molding alloy powder |
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